Browse Our Chemical Engineering Journals
Chemical engineering is an engineering branch that deals with the chemical production and manufacture of products that undergo chemical processes. This includes equipment design, creating systems and processes to refine raw material, as well as mixing, compounding, and processing chemicals to create products.
Chemistry and Chemical Engineering
Abstract
In our study, using a combination of eye-tracking parameter analysis and the van Westendorp method, we investigate whether participants pay more attention to products that they perceive as more expensive or to those that they prefer in the ranking process. The experiment involved 50 participants, a questionnaire with ranking and pricing tasks, and an eye-tracking measurement. Three wine varieties (Irsai Olivér, Rosé and Merlot-Shiraz) and three different label alternatives were tested. When comparing the results of the ranking and the pricing tasks, the product that is considered more expensive is not always the one that is most appealing to the participants. If we compare the results from the analysis of the eye-tracking parameters and the pricing, we can say that in all cases the labels that received the most visual attention were those that were priced more expensively by the participants.
Abstract
An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.
Abstract
A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank.
Abstract
The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R 2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument.
Abstract
Residues of the fungicides difenoconazole, propiconazole, cyflufenamid, and mandipropamid were determined in tomato fruit using acetonitrile for extraction and LC-MS/MS for quantification. Validation criteria include linearity range, the limit of detection (LOD) and limit of quantitation (LOQ), accuracy in terms of precision and trueness, and matrix effect were studied. The recovery rates of the method ranged from 91.8 to 106.3%. The precision of the method in terms of repeatability at one day (RSDr) and between three days (RSDR) ranged from 2.8 to 6.4% and from 4.3 to 7.6%, respectively, with good trueness from 92.2 to 96.4%. Matrix effects (suppression effects) ranged from 3.8% to 11.1%. The validated method was used to evaluate the dissipation kinetics of three different premix formulations: 30% EC (15% difenoconazole + 15% propiconazole), 14% DC (12.5% difenoconazole + 1.5% cyflufenamid), and 50% SC (25% difenoconazole + 25% mandipropamid) used on field tomatoes in Egypt. A first-order kinetic equation best describes residue dissipation. The calculated half-lives of difenoconazole, propiconazole, cyflufenamid, and mandipropamid were 2.01–2.27, 1.89, 1.97, and 1.71 days, respectively. The dissipation rate of difenoconazole did not differ significantly in the three premix formulations. Mandipropamid also dissipated faster compared to the other fungicides tested. The chronic dietary risk assessment results showed a minimal risk to adult Egyptian consumers. Waiting periods were advised for the safe consumption of tomatoes treated with the tested premix formulations.
Az azbesztszálak kimutatására szolgáló vizsgálatok középpontjában a levegőszennyezettségi értékek álltak, de a 21. században felmerült az igény a problémakör kiterjesztésére. Az elmúlt években megjelent nemzetközi tudományos szakirodalmak megcáfolták az évtizedeken át fennálló feltételezést, miszerint az azbeszt csupán a levegőterheltség révén vált ki kockázatot. Vízminőségi és talajminőségi kutatások által teret nyert az azbesztszálak, különösen a krizotilszálak alternatív transzportútjainak vizsgálatát célzó kutatásterület. Annak ellenére, hogy mind a települési, mind pedig a mezőgazdasági vízgazdálkodás potenciálisan érintett a krizotil-azbeszt jelenléte kapcsán, nincs nemzetközi szinten egységes és elfogadott módszer vagy küszöbérték az egyes vízforrások biztonságára vonatkozóan. A kutatások nyilvánvaló korlátja, hogy csekély mennyiségű és minőségű tudás érhető el. Az azbesztszálak megjelenése az egyes vízbázisokban jelentősen megváltoztatja mind a mezőgazdasági, mind a települési vízgazdálkodás környezeti hatásoknak való kitettségéről alkotott eddigi ismereteinket. Az öntözővizzel és a gyűjtött csapadékkal kijuttatott azbesztszálak hatásainak palettája mára túlhaladta a humán- és állategészségügyi hatásokat, immár figyelmet kell fordítani a vegetációs hatásokra is. Annak érdekében, hogy nagyobb betekintést nyerjünk az azbeszttoxicitás növényekre gyakorolt hatásaiba, sokkal több tudományos eredményre van szükség.
Jelen összefoglaló tanulmányban bemutatjuk az azbeszt, különös tekintettel a krizotil azbeszt legfontosabb tulajdonságait, humán-, állat- és növényegészségügyi kockázatait. Rávilágítunk arra, hogy ismereteink rendkívül hiányosak, valamint felhívjuk a figyelmet a települési és mezőgazdasági vízgazdálkodás érintettségének egyes faktoraira, közvetlen és közvetett kockázati tényezőire, valamint arra, hogy ezek miként hatnak az élőlényekre, kiemelt tekintettel a növényekre.
Abstract
A novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect.
Abstract
In this work, a UPLC-MS/MS assay was established for the determination of morphine, codeine, thebaine, papaverine and noscapine in rat plasma. ACQUITY UPLC BEH C18 column was employed for chromatographic separation with the mobile phase comprised acetonitrile-10 mmol L−1 ammonium acetate aqueous solution (0.05% aqueous ammonia) using gradient elution. Midazolam was used as internal standard (IS). Electrospray ionization (ESI) in positive-ion mode with reaction monitoring (MRM) was used for quantitative analysis. The calibration curves for morphine, codeine, thebaine, papaverine and noscapine demonstrated good linearity (r > 0.995) in the range of 5–500 ng mL−1 for morphine and codeine, and 1–100 ng mL−1 for thebaine, papaverine and noscapine. The intra-day and inter-day precisions of morphine, codeine, thebaine, papaverine and noscapine were within 15%, the intra-day and inter-day accuracies were 89–114%, the recovery was better than 65%, and the matrix effects were 96–112%. The developed UPLC-MS/MS assay was successfully applied in the pharmacokinetics of papaverine and noscapine.
Abstract
In this study, a UPLC-MS/MS method was developed for determination of pancratistatin in the mouse blood, and the pharmacokinetics of pancratistatin in mice after intravenous (5 mg kg−1) and intragastric (15 mg kg−1) administration was studied. HSS T3 column was used for separation with mobile phases of acetonitrile and 0.1% formic acid using gradient elution procedure. The blood sample was treated by protein precipitant with acetonitrile, midazolam was used as internal standard (IS). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, m/z 326.2→83.8 for pancratistatin and m/z 326.2→291.4 for IS in electrospray (ESI) positive interface. It showed a good linear in the range of 10–4,000 ng mL−1 (r > 0.998); the intra-day and inter-day precision was <15%, and the accuracy was 93%–105%. The recovery was better than 82%, and the matrix effect was 94%–105%. The developed UPLC-MS/MS method was fast, selective, and suitable for the pharmacokinetics of pancratistatin in mice.
Abstract
The rapid technological development that is still taking place today, with increasingly interconnected IT tools, is introducing dramatic changes. The development of computer programs is rapidly transforming traditional processes and the systems that support them. It is therefore natural that the fourth industrial revolution (Industry 4.0) and its impact on Hungarian companies is one of the key topics of our time. We conducted an exploratory quantitative survey, asking 140 managers of Hungarian small, medium and large enterprises about their current situation in the context of Industry 4.0. We sought to find out to what extent the specific R&D and innovation potential of Industry 4.0 is accepted, and whether it has already been introduced in the companies. On a qualitative side, 2 case studies and 3 interviews were conducted, in which structured interviews were used to further explore the issue. We aimed to find out where SMEs stood in terms of digital preparedness and what advantages, possible disadvantages, and goals they managed to identify. Our research showed that an increasing number of companies have already decided to take the first steps towards industrial digitalisation, which will completely transform their internal processes.
Abstract
A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250 mm × 4.6 mm, 5 µm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL·min−1 and a column temperature of 40 °C. The drift tube temperature of the evaporative light scattering detection system was set at 40 °C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r = 0.9993–0.9995) during the test ranges (119.1–1190.7 μg·mL−1 for 12-hydroxystearic acid, 10.7–107.4 μg·mL−1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg·mL−1, the limits of quantitation were 3.2 and 7.4 μg·mL−1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n = 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.
Abstract
Indapamide (Indp) and certain other diuretics have been abused in sports, therefore, having sensitive methods for its detection and assay in biological fluids (whole blood, plasma, serum, and urine) is of significant importance. The racemic mixture of Indp is being used as an active pharmaceutical ingredient among other commonly prescribed diuretics. The regulatory authorities and pharmaceutical industries demand analytical methods for successful enantioseparation of such molecules. The paper presents a critical overview of the scientific issues of the application of contemporary techniques involving various chromatographic approaches (with liquid or supercritical fluid as mobile phases) and capillary electrophoresis and method development, for drug screening, assay, bioequivalence studies and enantioseparation of indapamide with their results. It also covers the historical developments that led to significant breakthroughs in research and concise evaluations of research in the area.
Different types of chromatographic methods (HPLC, CEC, SFC etc) discussed herein provide an insight and a choice to select a method to (i) screen Indp for drug abuse, (ii) separate, isolate and quantify the enantiomers of Indp and (iii) investigate their pharmacokinetics as markedly different species and not as a total drug. The article evaluates the field's status with a broad base and practical oriented approach so that the underlying principles are easily understood to help chemists and non-specialists gain useful insights into the field outside their specialization and provide experts with summaries of key developments. To the best of authors' knowledge there has been no attempt to review such methods for analysis of Indp and this is the first report of its kind.
Rambutan (Nephelium lappaceum) production is growing worldwide so the treatment and utilization of Rambutan by-products has become a concern of manufacturers. The objective of this study was to evaluate the potential application of rhizobacteria to decompose Rambutan peel for organic fertilizer production. After the rhizospheric soil samples were selectively proliferated and preadded on agar medium containing only Rambutan peel, the rhizobacterial colony isolates were screened based on their ability to grow on this agar medium and then to degrade cellulose in Rambutan peel. The LD7.3 isolate from the Rambutan rhizosphere showed the highest efficiency in degrading Rambutan peel with 5.6% degraded cellulose content and was identified by the MALDI-TOF technique as belonging to Klebsiella. Klebsiella sp. LD7.3 grew well and maintained the same degrading activity after three times of subculturing in liquid medium. Notably, the supplementation of grinded Rambutan fruit peel to the liquid medium had a positive effect on the growth and the degrading activity of Klebsiella sp. LD7.3. This was the primary report on the application of rhizobacteria to degrade Rambutan peel and the results showed that this was a potential approach to reuse this waste source.
The experiment was conducted within a framework of a two-factor long-term trial at the Research Institute for Fisheries, Aquaculture and Irrigation, in Szarvas, Hungary. This was a special field experiment, in which lysimeters have been installed in the middle of 32 m2 field plots. The main factor was the water supply with 4 levels: i1: non-irrigated control; i2: irrigated with one third of the optimal water supply; i3: irrigated with two thirds of the optimal water supply; i4: optimum irrigated plot, according to the requirement of sweet corn test plant. The amount of released irrigation water was 0, 54, 106 and 158 mm per year on average over 5 years. Within every water supply treatment there were 4 nutrient supply rates (N): N1, N2, N3, N4 = 100, 200, 300 and 400 kg ha−1 NPK fertiliser substance in ratio 2:1:1. The number of replications was 4, and the experiment was arranged in split-plot design. In the studied years, the amount of precipitation varied between 92 and 264 mm from sowing to harvesting.
The effect of fertiliser was less in the non-irrigated treatments compared to that of the irrigated ones, and the yield was increased only up to 200 kg ha−1 NPK treatment level. The NPK dose of 300 kg ha−1 proved to be optimal in the irrigated treatments in which the utilization of fertilizer doses increased parallel to the improving water supply. In addition, the ratio of first class products (cobs longer than 20 cm) increased to a greater extent than the yield as a result of irrigation and fertilization. Water requirement of sweet corn proved to be between 400–450 mm resulting in an average yield of 20–24 t ha−1, of which 18–20 t ha−1 came from marketable cobs. The amount of evapotranspiration fluctuated between 270–440 mm during the five years, depending on the quantity of water supply, but it changed to a lesser extent than the amount of the yield. Increasing the fertilizer dose practically did not affect ET in non-irrigated plants, but increased it by 20–30 mm in irrigated ones. The change was not significant.
The productivity of ET was only 30–45 kg ha−1 mm−1 in the non-irrigated treatment, while it was 50–55 kg ha−1 mm−1 in the irrigated treatments, with higher values at the higher fertiliser rates. The productivity of irrigation water exceeded far over the productivity of ET at adequate nutrient supply. The yield increase per 1 mm of irrigation water was on average 60 kg ha−1 mm−1, which was considerably higher than the productivity of ET of non-irrigated plants (39 kg ha−1 mm−1). There was a positive correlation between the yield and ET, and a negative correlation between the yield and specific water consumption. Irrigation and fertilization increased the average yield to a greater extent than evapotranspiration, so as the average yield increased, the ET per unit of yield decreased, i.e. the productivity of evapotranspirated water increased.
Abstract
Pregabalin is a gabapentinoid approved for the treatment of general anxiety disorder, neuropathic pain and as adjunctive therapy for focal seizures in patients with epilepsy. In addition, there are a number of conditions for which pregabalin is prescribed off-label. Along with the widespread use there are a significant number of reports describing the misuse of pregabalin over the last decade. Over time, it became clear that pregabalin should become part of routine testing in toxicology laboratories. The aim of this paper was to present validation of a LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients. Simple sample preparation step and rapid chromatographic separation shortened the overall analysis time, which was the goal of method development. The presence of pregabalin was confirmed with three ion transitions, ensuring high selectivity of the validated method. The statistical data obtained showed good precision and accuracy over a wide concentration range. No endogenous or other interference was detected, and there was no matrix effect influence with this method. The LC-MS/MS method was applied to quantify pregabalin in plasma samples of patients admitted to the emergency department due to a possible acute pregabalin overdose. Different concentrations were found, and we report, to the best of our knowledge, the highest plasma concentration of pregabalin in the plasma of a patient with acute poisoning. In conclusion, we developed a fast and simple LC-MS/MS method for reliable determination of pregabalin and demonstrated the developed method was suitable for routine use in clinical toxicology setting.
Abstract
Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants (POPs) that are widely distributed in the environment and cause significant environmental damage. Furthermore, they endanger human health by polluting food from the natural environment and food processing. Therefore, it is necessary to accurately detect PAHs in various sample matrices, which requires precise, practical, and rapid detection methods. The purpose of this research is to develop a high sensitivity analysis method by analyzing the optimum excitation and emission wavelengths of EPA's 15 priority polyaromatic hydrocarbons in the UHPLC fluorescence detector (Acenaphthene, Anthracene, Benzo[a]anthracene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Benzo[ghi]perylene, Benzo[a]pyrene, Chrysene, Dibenzo[a,h]anthracene, Fluoranthene, Fluorene, Indeno[1,2,3-cd]pyrene, Naphthalene, Phenanthrene, and Pyrene). An average of 17–25 analyses were performed for each polyaromatic hydrocarbon, and optimized excitation and emission wavelengths were obtained. LOD levels between 2 and 90 ppt were obtained with the method created in this direction. It is worth mentioning that the limits achieved for some PAH parameters are lower than those reported in the literature after pre-concentration steps.
Abstract
The two chemical components Escitalopram (ESC) and Etizolam (ETZ) are beneficial for the health of individuals because it helps to treat anxiety. The study mainly illustrated that a green approach is essential in the medical sector with the help of “Green Analytical quality by design”. According to AQbD, the techniques of HPTLC have become eco-friendly, and decided to use “ESC” and “ETZ”. Hence, ethanol and phosphate buffer pH 3.5 adjusted with 1% “orthophosphoric acid”. After the retardation factor, the product ESC was found at 0.34 min and ETZ was found at 0.53 min. The linearity of ETZ the range varies from 300 to 1800 μg mL−1 and for ESC it varies from 100 to 600 μg mL−1. The validation parameter of R 2 Values ranged from 0.9997 to 0.9994 for both ESC and ETZ. The study also demonstrated that different other methods were also useful for the medical sector to make it more convenient and eco-friendly. Some of those approaches are “GAPI”, “AGMS”, “NEMI”, and “AGREE”. The outcome of the study helped to find that the technique “HPTLC” is a green analytic design that helps to maintain the stability of the medicine and it was also approved as a quality design and also a novel approach in the pharmaceutical sector.
Abstract
Using the Design of Experiments methodology (Response-Surface Methodology and Derringer's Desirability Function), a simple, fast and robust RP-HPLC method was developed for the analysis of enrofloxacin (EFC), its impurity A (fluoroquinolonic acid, FQ) and impurity B (ciprofloxacin, CPX). Gradient elution of samples was performed on a Zorbax Eclipse XDB C18 column (150 × 4.6 mm, 3.5 μm) with a mobile phase consisting of 32 mM phosphate buffer pH 3.5 – methanol (0 min-19.6% methanol; 15.5 min-19.6% methanol; 29.5 min-80% methanol; 30 min-19.6% methanol; 35 min-19.6% methanol), delivered at a flow rate of 1.5 mL min−1, wavelength of detection 278 nm (for EFX and CFX) and 265 nm for FQ. A good linear response was achieved in the range 15–35 μg mL−1 (EFX) and LOQ-150% for impurities (CFX and FQ). Other validation parameters were also tested: precision, accuracy, sensitivity and robustness. The developed method was shown to be simple, practical and suitable for the analysis of EFC and its impurities (CPX, FQ) in veterinary drugs.
Abstract
A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.
Abstract
SZJ-1207 is an antidepressant natural product with a steroidal structure extracted from Stephanotis mucronata. It is a novel antidepressant candidate molecule and all its pharmacokinetic properties have not been reported. In this pharmacokinetic study in mice following oral administration, an accurate and sensitive UPLC-MS/MS method was established and evaluated to measure SZJ-1207 concentrations in mouse plasma and brain samples. The results provide information regarding the pharmacokinetics of SZJ-1207 as a potential antidepressant.
Az „Alsóban az élet” című hazai talajállapotot célzó közösségi tudomány program első tapasztalatai és eredményei
The First experiences and results of the Hungarian citizen science program (’Life in Undies’) aimed at soil properties
A közösségi tudomány – citizen science – már évtizedek óta működő kutatási forma, ahol egy-egy kutatás a lakosság segítségével valósul meg. Az „Alsóban az élet” kampány az érdeklődők bevonásával 2021 tavaszán indult hazánkban. A kutatásban résztvevők kézhez kaptak egy pamut alsóneműt, amelyet kb. 20 cm-es mélységben kellett elásniuk, ezzel „táplálékot” szolgáltatva a talajlakó élőlények számára. Több mint két hónap elteltével az alsónemű kiásása után megfigyelhetők a bomlási jelek, amelyek mint indikátor jelzik a talajélet aktivitását, közvetett módon a talaj egészségi állapotát. A visszamaradt alsóneműk digitális fotójának elemzésével becsülhető a talajlakó élőlények munkája az alsónadrágok bomlásának százalékos aránya alapján.
A közösségi médiában megjelent felhívások és célzott csoporthirdetések segítségével mintegy 1193-an jelentkeztek a programra összesen 1966 helyszínnel, ezzel országos lefedettséget biztosítva a kutatás részére. Az adatok elemzése alapján a gondozott konyhakertekben elásott pamut alsók mutatták a legnagyobb átlagos bomlási értékeket (27,67%). Talajtípust tekintve a réti talajok és a közép- és délkeleteurópai barna erdő-, valamint a csernozjom-, és a váztalajok (köztük nagyrészt a humuszos homoktalajok) esetén tapasztaltuk a legmagasabb, közel azonos, 25,47%; 25,43%; 24,22%; 24,21%-os bomlási értéket. A programban résztvevő helyszínek közül a legnagyobb mértékű bomlás (93%) konyhakert hasznosítású (mulcsozott veteményes és polikultúra ágyás) váztalajon (homoktalajon) volt megfigyelhető. Az országos átlagos bomlási érték 24,57% volt. A bomlási adatok alapján eredménytérképet szerkesztettünk Magyarország teljes területére, melyet nyilvánossá tettünk, s a résztvevőknek a visszaküldött fotó feldolgozása alapján rövid, a saját talajának biológiai aktivitását minősítő válaszlevelet küldtünk.
Abstract
The retention behaviour of scopolamine (hyoscine) and its related compounds (norhyoscine, atropine, homatropine, and noratropine) was investigated on the silica-based HPLC stationary phase. The retention of investigated tropane alkaloids was interpreted by using the Soczewiński-Wachtmeister equation. A high correlation between the retention parameter (log k) and lipophilicity (log P) (R = 0.9923) confirms the significant influence of hydrophobic interactions on the retention behaviour of the aforementioned compounds. It was found that by increasing the acetonitrile fraction, a decrease in retention of the more polar epoxide derivatives (scopolamine, norhyoscine) and an increase in retention of the more lipophilic derivatives (atropine, noratropine, homatropine) is obtained. The best separation of the tropane alkaloids was achieved by a simple procedure that involved a mobile phase composed of acetonitrile and 40 mM ammonium acetate/0.05% TEA, pH 6.5; 50:50 v/v. Selected conditions were assumed for the determination of scopolamine hydrochloride in the eye drops (Scopolamini hydrobromidum 0.25%). The method was validated and it was found as selective, sensitive, precise, accurate, and robust for the further qualitative analysis of the scopolamine-related compounds.
Abstract
In this study, we report the systematic approach for characterization of two major degradant impurities, which are not listed in any compendia and were formed during the stability studies of Dihydroergotamine mesylate injection (DHE). An ion-pair UPLC chromatographic method was developed to quantify the related substances present in the DHE injection drug product. The same was used to monitor the impurity profiling during its stability. The two unknown impurities were observed at RRT about 0.08 (Impurity-1) and RRT about 0.80 (Impurity-5) and found to be significantly increasing on stability. Forced degradation studies revealed the nature of the impurity and conditions required for enriching them. A Mass compatible HPLC method was developed to quantify only these two impurities using 25% ammonia and formic acid in water. Their mass numbers were identified using LC MS/MS with triple quadruple mass spectrometer coupled with a HPLC. These two impurities were then isolated from enriched products using preparative HPLC. These impurities were then characterized using Mass and NMR analysis along with Q-TOF elemental analysis.
Abstract
Bacterial DNA gyrase and topoisomerase IV control the topological state of DNA during replication and represent important antibacterial drug targets. To be successful as drug candidates, newly synthesized compounds must possess optimal lipophilicity, which enables efficient delivery to the site of action. In this study, retention behavior of twenty-three previously synthesized dual DNA gyrase and topoisomerase IV inhibitors was tested in RP-HPLC system, consisting of C8 column and acetonitrile/phosphate buffer (pH 5.5 and pH 7.4) mobile phase. logD was calculated at both pH values and the best correlation with logD was obtained for retention parameter φ0, indicating that this RP-HPLC system could be used as an alternative to the shake-flask determination of lipophilicity. Subsequent QSRR analysis revealed that intrinsic lipophilicity (logP) and molecular weight (bcutm13) have a positive, while solubility (bcutp3) has a negative influence on this retention parameter.
Hígtrágya komplex baktérium-kezelésének hatása egyes beltartalmi és ökotoxikológiai tulajdonságokra
The effect of complex bacterial treatment of slurry on content and ecotoxicological properties
Kutatásunk témája az NCH Magyarország Kft. által forgalmazott baktériumos hígtrágyakezelési rendszer összehasonlító ökotoxikológiai vizsgálata. A kísérletet egy szarvasmarha borjúnevelő telepen végeztük 0–6 hónapos korcsoportú szekcióban. A tabletta formában rendelkezésünkre álló baktérium törzseket egy tartályban felszaporítottuk és hetente adagoltuk az aknában összegyűlő hígtrágyához. A kezelés célja volt, hogy a baktériumok elősegítsék a trágya homogenizációját, a szagcsökkentést és a szerves szennyeződések lebontását. Az ökotoxikológiai vizsgálatokat a trágyakezelés előtt, alatt és után, három mintavételi időben végeztük el.
A kutatásunk eredményeként elmondhatjuk, hogy a hígtrágyakezelés során a beltartalmi értékek jelentősen növekedtek, főként a nitrogénformák, a biológiai oxigénigény és a szárazanyagtartalom. Az ösztrogén hatás megléte számottevő maradt a kezelés végére is. A fitotoxicitási vizsgálat alapján mindegyik növény, szár- és gyökérnövekedésére pozitív hatással volt a trágyakezelés. A talajtoxicitási teszt eredménye bizonyította, hogy magasabb hígítás mellett veszti el a kezeletlen hígtrágya az érzékeny baktériumok élettevékenységére is kiterjedő gátló hatását. A békalencse vizsgálat során összességében elmondható, hogy 150× hígítás fölött megszűnik a hígtrágya gátló hatása mindhárom alkalommal vett minta esetében. Az alga növekedésgátlására a hígtrágya stagnáló-gátló tendenciát mutatott a kezelés alatt.
Eredményeink alapján arra a következtetésre jutottunk, hogy a vizsgált hígtrágyakezelési módszer a homogenitás, szagtalanítás és a szerves anyagok bontása során eredményes volt. Azonban javasolt magasabb hígítási arányban vagy magas talajvíztartalom mellett kijuttatni a földekre. A hormonhatású anyagok eltávolítására vonatkozólag további vizsgálatok szükségesek, melyek alapján majd javaslatokat lehet kidolgozni a gazdák számára.
Abstract
Rationale
The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects.
Methods
An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C18 column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min−1. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source.
Results
In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control.
Conclusions
A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.
Abstract
We developed and validated a sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry (2D-LC‒MS/MS) method to determine the concentration of mometasone furoate in human plasma after nasal spray administration. Isotopically labeled mometasone furoate-13C,d6 was used as an internal standard (IS). Plasma samples were prepared using a solid-phase extraction (SPE) method. With this 2D-LC strategy, the analytes were trapped in the first dimension (1D) column, and only judiciously selected portions of the 1D effluent were transferred to the second dimension (2D) column for further separation to obtain high-resolution information. MS/MS quantification was performed in positive ionization mode via multiple-reaction monitoring (MRM). This analytical method was fully validated according to related regulatory guidance, and the results showed that the method is robust and sensitive enough for pharmacokinetic investigation of mometasone furoate with satisfactory linearity from 0.25 to 30 pg mL−1. This method was successfully applied to a bioequivalence (BE) study of mometasone furoate aqueous nasal sprays in healthy volunteers.
Abstract
A simple, rapid, sensitive and eco-friendly liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of free cordycepin (3′-deoxyadenosine) and isocordycepin (2′-deoxyadenosine) in 10 kinds of Cordyceps samples. The samples were prepared by ultrasonic extraction at 75 °C for 30 min with boiling water as the extraction solvent. The LC separation was performed on an Agilent poroshell 120 SB-Aq C18 column (3.0 × 50 mm, 2.7 μm) in isocratic mode with an eco-friendly mobile phase (2% ethanol containing 0.2% acetic acid) at a flow rate of 0.6 mL min−1, and detected by MS/MS in positive mode with multiple reaction monitoring (MRM). The developed method showed good linearity (r > 0.9990), sensitivity (LODs = 0.04 pg, LOQ = 0.1 pg), precision (RSD ≤ 3.8%) and stability (RSD ≤ 3.6%). The recoveries of developed method were 94.4–109.5% (RSD ≤ 5.5%). Compared with reported methods, the current method was rapid (less than 35% analytical time), sensitive (more than 5 folds), and eco-friendly (less than 10 μL harmful organic solvent). 10 different kinds of Cordyceps samples (40 batches) were tested by the developed method. Codycepin was only found in Cordyceps millitaris and C. millitaris fruiting body, and isocordycepin was detected in Cordyceps sinensis and other 6 Cordyceps samples. The developed method would be an improved method for the quality evaluation of Cordyceps samples.
Abstract
The study was aimed to validate and optimize high performance liquid chromatographic (HPLC) method for the determination of coumarin-3-carboxylic acid (C3A) in the heart and liver issue of Sprague-Dawley (SD) rats after intragastric administration of extractive of leaves of Ficus virens var sublanceolata. And simple ADME and target prediction analyses were performed for C3A. Ethyl acetate was employed to precipitate protein with appropriate sensitivity and acceptable matrix effects. The satisfactory separation was developed on an ODS2 column (4.6 mm × 250 mm, 5 μm) by gradient elution with a methanol-acetic acid solution (pH = 3.0) as the mobile phase. The flow rate was 1.0 mL min−1, the column temperature was maintained at 30 ± 2 °C, the injection volume was 20 μL, and the detection wavelength was set as 309 nm. The method was fully validated in terms of selectivity, linearity, accuracy, precision, extraction recovery and stability. The results of the ADME analysis found that C3A has excellent characteristics of drug-likeness, consistent with good bio-absorption. And the predicted 12 target protein belongs to the amine oxidoreductase and carbonic anhydrase target class. This method is simple, rapid, sensitive, and accurate for the determination of coumarin-3-carboxylic acid in the heart and liver tissue of SD rats.
Húsz éves avarmanipulációs kísérlet hatásai barna erdőtalaj szén tartalmára és vízkapacitására: Síkfőkút DIRT Project
The effects of a twenty-year litter manipulation experiment on the carbon content and water retention capacity of the examined Luvisols: Síkfőkút DIRT Project
A talajok a szárazföldi széntároló rendszerek egyik legjelentősebb tagját jelentik, melyek szénelnyelése, illetve szénkibocsátása jelentős mértékben hat a klímára, ugyanakkor a klímaváltozás is befolyásolja a talajok szénraktározó képességét. Az avar produkció mennyiségi és minőségi változásai jelentősen befolyásolják ezeket a folyamatokat, azonban ezek mértéke, sőt időnként iránya sem ismert pontosan.
A klímaváltozás mellett a területhasználat változások is befolyásolják a talajba kerülő szerves anyagok mennyiségét és ezen keresztül számos egyéb talajfizikai, kémiai és biológiai paramétert. Ezeknek a hatásoknak a rendszerszintű vizsgálatát segítik a nemzetközi avarmanipulációs projektek, melyek azonos kezeléseket alkalmazva, de eltérő klímaviszonyok mellett vizsgálják a mesterségesen átalakított avar inputok hatását a talajrendszerekre. A Síkfőkút project területén, mely 2000-ben csatlakozott a nemzetközi DIRT projecthez, vizsgáltuk az avar input növekedésének és csökkenésének hatásait egy cseres tölgyes erdőben a talajok szén körforgalmára, illetve a vízháztartására. Ezeken a kutatásokon belül vizsgáltuk a kezelések talajaiban a talajnedvesség tartalmat, vízkapacitást és térfogatsűrűséget, valamint CNS analizátorral a talajok szerves szén tartalmát.
Eredményeink azt mutatták, hogy az avar produkció mennyiségi változása, éghajlati viszonyoktól függően, eltérően hat a talajok SOC tartalmának változásaira. A kezelésekkel modellezett avar produkció változások nemcsak közvetlen úton hatnak a talajok szerves anyag tartalmára, de közvetett módon a megváltozott mikroklimatikus viszonyok révén is befolyásolják a talajok szén és vízforgalmi viszonyait. A nagyobb avar produkció a szárazabb síkfőkúti erdőben növelte a talajok szén tartalmát (szemben a nedvesebb amerikai területeken tapasztalt visszaeséssel, vagy stagnálással) és magasabb szerves anyag tartalom társulva a vastagabb avartakaróval magasabb átlagos talajnedvességet és vízmegtartó képességet eredményezett az avar elvonásos kezelésekkel szemben. Ezek a hatások összefüggésben lehetnek azzal is, hogy az avarelvonásos kezeléseknél szignifikánsan magasabb térfogattömeg értékeket mértünk, ami a pórustérfogat csökkenését jelentheti ebben az esetben, csökkentve ezzel a talajban tárolható víz mennyiségét.
Az általunk végzett avarmanipulációs kísérletek nemzetközi kontextusában közelebb juthattunk a biogeokémiai ciklusok, ezáltal a mineralizáció és a humifikáció közötti összefüggések megértéséhez különböző erdőtípusokban és különböző klimatikus feltételek között.
Abstract
In the present study, an LC-MS/MS method allowing to quantify pretomanid and pyrazinamide simultaneously in rat plasma was developed. Chromatographic separation was achieved on an Agilent Eclipse plus C18 column (100 mm × 2.1 mm, 3.5 μm; Agilent, USA) and maintained at 30 °C. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 360.1 → m/z 175.1 for pretomanid, m/z 124.1 → m/z 81.0 for pyrazinamide, m/z 172.1 → m/z 128.1 for metronidazole (IS). The calibration curves showed good linear relationships over the concentration range of 50–7,500 ng mL−1 for pretomanid and 500–75,000 ng mL−1 for pyrazinamide. The precision and accuracy were below 15% and within ±15% of the nominal concentrations, respectively. The selectivity, recovery and matrix effect of this method were all within acceptable limits of bioanalytics. The method was applied to the analysis of plasma samples from pharmacokinetic studies in rats. The results show that the main pharmacokinetic parameters of pyrazinamide, namely, T max, t 1/2, and AUC(0–t), decreased in the combined group than in the alone group.
Abstract
Muscle relaxants and pain killers with their different types are widely used as combination approach for treatment of pain associated with several muscle spasm conditions. A sensitive and simple HPLC-UV detection method was developed in this work for simultaneous assay of Dantrolene (DNT) and co-administrated: Ibuprofen (IBU) and Diclofenac (DIC). After simple protein precipitation, separation was achieved using C18 column (150 × 4.6 mm) with a mobile phase of acidified water with orthophosphoric acid (pH = 3.5) and acetonitrile using gradient elution with a flow rate of 1 mL/min. The DAD was adjusted at 380, 219, 280 and 240 nm to measure DNT, IBU, DIC, and dexamethasone (internal standard), respectively. Linearity was demonstrated over the range from 0.1 to 3 μg/mL, 1 to 40 μg/mL, and 0.1 to 2 μg/mL for DNT, IBU, and DIC, respectively. The validated method was applied successfully to compare the effect of co-administration of IBU or DIC on the pharmacokinetic profile of DNT.
Abstract
70 species of grasses family (Poaceae), coming from genera: Agrostis, Alopecurus, Anthoxanthum, Apera, Arrhenatherum, Avena, Brachypodium, Briza, Bromus, Calamagrostis, Corynephorus, Cynosurus, Dactylis, Danthonia, Deschampsia, Digitaria, Echinochloa, Elymus, Eragrostis, Festuca, Glyceria, Helictotrichon, Hierochloe, Holcus, Hordeum, Koeleria, Leymus, Lolium, Milium, Molinia, Nardus, Panicum, Phalaris, Phleum, Phragmites, Poa, Saccharum and Setaria, collected mostly from natural stands in Poland during 2020 season, were subjected to GC-MS fingerprinting of headspace volatile fraction above dried material. Obtained mass spectrometry data were analyzed by means of principal component analysis (PCA) and hierarchical cluster analysis (HCA). Five species: Glyceria maxima (Hartm.) Holmb., Lolium multiflorum Lam., Hordeum jubatum L., Bromus tectorum L. and Bromus secalinus L. were identified as outliers, which is consistent with our earlier analysis by thin layer chromatography. These species deserve further look and their outliance is orthogonal to coumarin content, which was independently observed for odorant species of grasses.
Abstract
If we want to increase the efficiency of precision technologies to create sustainable agriculture, we need to put developments and their application on a new footing; moreover, a general paradigm shift is needed. There is a need to rethink close-at-hand and far-off innovation concepts to further develop precision agriculture, from both an agricultural, landscape, and natural ecosystem sustainability perspective. With this, unnecessary or misdirected developments and innovation chains can be largely avoided. The efficiency of the agrotechnology and the accuracy of yield prediction can be ensured by continuously re-planning during the growing season according to changing conditions (e.g., meteorological) and growing dataset. The aim of the paper is to develop a comprehensive, thought-provoking picture of the potential application of new technologies that can be used in agriculture, primarily in precision technology-based arable field crop production, which emphasizes the importance of continuous analysis and optimisation between the production unit and its environment. It should also be noted that the new system contributes to reconciling agricultural productivity and environmental integrity. The study also presents research results that in many respects bring fundamental changes in technical and technological development in field production. The authors believe that treating the subsystems of agriculture, landscape, and natural ecosystem (ALNE) as an integrated unit will create a new academic interdisciplinarity. ICT, emphasizing WSN (Wireless Sensor Network), remote sensing, cloud computing, AI (Artificial Intelligence), economics, sociology, ethics, and the cooperation with young students in education can play a significant role in research. This study treats these disciplines according to sustainability criteria. The goal is to help management fulfil the most important expectation of reducing the vulnerability of the natural ecosystem. The authors believe that this article may be one of the starting points for a new interdisciplinarity, ALNE.
Abstract
An easy, quick, and sensitive approach adopting ultra-performance liquid chromatography (UPLC) equipped with diode array detector was used to analyze and systematically evaluate the quality of Pudilan tablets manufactured by 12 distinct pharmaceutical companies. In this research, 15 peaks were chosen as the common peaks to assess the similarities for different batches (S1–S43) of Pudilan tablet samples. In comparison with the control fingerprint, similarity values for 43 batches of samples exceeded 0.922. In addition, by analyzing the reference substances of epigoitrin, caffeic acid, chlorogenic acid, acetylcorynoline, baicalin and baicanshialein, the chromatogram of the 6 reference substances was established. The recoveries for the reference substances which demonstrated good regression in the linear range (r 2 > 0.999) were in the range of 98.3–101.1%. The results demonstrated that the established method was highly accurate, efficient and reliable. This study provides a valid, dependable and pragmatic method to evaluate the quality of Pudilan tablet.
Szántóföldi szénmérleg egy közép-magyarországi mintaterületen
Carbon balance of a cropland site in Middle-Hungary
2017. októberétől 2021. októberéig terjedő időszakban vizsgáltuk egy középmagyarországi szántóföld szénforgalmát gázcseremérések segítségével. A mért nettó ökoszisztéma gázcsere (NEE) adatokból kumulált összegeket számoltunk éves bontásban, illetve az egyes növényállományok és ugar időszakok szerint. Gazdálkodási adatok segítségével számoltuk a területre behozott (import) és onnan elvitt (export) szénmennyiségeket, valamint az NEE, az import és az export áramokat összesítve szénmérleget (NECB) számítottunk az NEE összegekhez hasonló bontásban.
Az eredmények alapján a szántóföld minden évben szénelnyelőnek bizonyult, annak ellenére, hogy a vizsgált időszak során több vízhiányos periódus is hátráltatta a növények megfelelő fejlődését és ezzel a szénfelvételt. A mért éves átlagos NEE összeg –69,6 g C m–2 év–1 volt. Ezzel szemben a teljes – laterális áramokat is tartalmazó – szénmérleg minden évben és minden növényállomány esetében veszteségesnek bizonyult, átlagosan –168 g C m–2 év–1 volt a szénveszteség mértéke. Ennek a deficitnek a jelentős része a vízhiányos időszakok alatti lecsökkent szénfelvételnek köszönhető, ezt jól mutatja a két őszi búza állomány szénmérlege közötti 66 g C m–2-es különbség, ahol az első állomány jó vízellátás mellett, a második pedig vízhiányos időszak alatt fejlődött. Nedvesebb időszakban vélhetően kevésbé jelentős a szénveszteség mértéke.
A szakirodalom alapján nincs olyan módszer, amellyel önmagában kompenzálni lehet egy ilyen mértékű veszteséget, azonban több olyan eljárás is létezik, amelyek kombinációjával jó eredményeket lehet elérni. Fontos lenne a hazánkban jól alkalmazható módszerek feltárása és azok szénmérlegben játszott szerepének számszerűsítése.
Koncepcióváltás a belvízgazdálkodásban: talajtani és vízminőségi kérdések
Conceptual Change in Excess Water Management: Soil and Water Quality Issues
Munkánk során igyekeztünk a belvízminőséggel, annak időbeli változásaival kapcsolatos kérdéseket megválaszolni.
Az eddig vizsgált nehéz agyag talajtextúrájú algyői mintaterületről származó eredmények rávilágítanak arra, hogy tápanyagok tekintetében számottevő terhelés érheti az elvezetés során a belvizet befogadó felszíni víztestet különösen a belvízelöntés kezdeti időszakában. A terhelést kiemelten a lebegőanyaghoz kötött tápanyagformák adják, míg emellett a felszíni vízborítás kialakulását követő első napokban és hetekben jelentős, környezetvédelmi határértéket is átlépő mineralizált nitrogéntartalomra is kell számítani.
A belvizes környezet reduktív jellemzőinek erősödésével a nitrát – külső utánpótlás nélkül – hamar átalakul, míg a hőmérséklet és a biológiai aktivitás emelkedésével a lebegőanyagtartalom koagulációja és flokkulációja is jelentősen csökkenti a tápanyagterhelést.
Ezen a mintaterületen képződött belvíz öntözővízként való hasznosítását az öntözőrendszer eltömődéséhez vezető magas lebegőanyagtartalom, illetve esetenként magas vas- és mangántartalom nehezítheti jellemzően szintén a tavaszi időszakban, amikor pl. kelesztő öntözéshez használhatjuk fel a vizet a magasabb térszíneken.
Általános érvényű következtetések levonásához a kutatás későbbi szakaszában két új, eltérő talajtani és hidrológiai adottságú mintaterületre is kiterjesztjük vizsgálatunkat. A helyszíni mérésekkel párhuzamosan összeállítunk egy laboratóriumi kísérletet kiemelten a talajtényező hatásának megfigyeléséhez. Ez lehetőséget fog nyújtani arra is, hogy a tápanyagformák időbeli átalakulásáról is pontosabb képet kapjunk.
Abstract
Codonopsis Radix (CR) is recorded as the roots of Codonopsis pilosula, C. pilosula var. modesta and Codonopsis tangshen. It is difficult to evaluate the quality of CR because of the existence of many original plants. In this paper, a strategy integrating chromatographic analysis and chemometrics for the quality control of CR is proposed. Systematic analysis of the chemical composition of CR was achieved through high performance liquid chromatography (HPLC) fingerprinting. Based on the HPLC fingerprinting data, chemometrics, including unsupervised principal component analysis (PCA) and supervised orthogonal partial least squares-discrimination analysis (OPLS-DA), were applied to classify all CR samples. Components with variable importance in projection values higher than 1 in the OPLS-DA model were selected as potential chemical markers for distinguishing the origins of CR. Finally, an HPLC method was validated for determining the five characteristic ingredients in the CR samples. HPLC characteristic fingerprints showed 17 common peaks for C. pilosula, 13 for C. pilosula var. modesta, and 9 for C. tangshen, and all of them showed good similarity (>0.9). Additionally, there were 9 common peaks for all CR samples with relatively poor similarity, ranging from 0.607 to 0.970. PCA could differentiate CR from the three origins, except for a partial overlap between C. pilosula and C. pilosula var. Modesta, and the OPLS-DA model achieved excellent classification results. Eight components (peaks 12, 8, lobetyolin, 10, codonopsin І, syringin, 3, and 11) were selected as potential chemical markers. There was a large discrepancy in the contents of the five characteristic ingredients in all samples, with the relative standard deviation ranging from 36.0% (lobetyolin) to 85.9% (atractylenolide Ⅲ). The average contents of the five characteristic ingredients were similar between C. pilosula and C. pilosula var. modesta samples and notably higher than those of C. tangshen samples. Consequently, a rapid, precise, and feasible strategy was established for the discrimination and quality control of CR with different origins.
Abstract
Bai-Hu-Jia-Ren-Shen-Tang Decoction (BHJRSTD) is one of the oldest classic Chinese medicine prescriptions which used in the field of treatment of diabetes. However, to the best of our knowledge, the ingredients of this prescription have not been identified, and there are very few studies on the anti-diabetic mechanism of this prescription. Therefore, BHJRSTD was detected and identified by ultra-high-performance liquid chromatography coupled with Quadrupole-Exactive Focus Orbitrap MS (UHPLC–Q/Orbitrap/MS/MS). We identified 74 compounds, including flavonoids, alkaloids, chalcones, xanthones, phenols, phen